Synthesis of bis(thio-hydrazide amide) salts
US7709683B2 · kind B2 · utility
Assignee
Inventors
Key dates
| Filing date | May 11, 2006 |
| Grant date | May 4, 2010 |
| Priority date | — |
| Expiry date | Aug 25, 2026 |
Classification
- Technology area (CPC C)Chemistry; Metallurgy
- CPC primaryC07C2601/14
- WIPO fieldOrganic fine chemistry
- WIPO sectorChemistry
Abstract
A method of preparing a bis(thio-hydrazide amide) disalt includes the steps of combining a neutral bis(thio-hydrazide amide), an organic solvent and a base to form a bis(thio-hydrazide amide) solution; and combining the solution and methyl tert-butyl ether, thereby precipitating a disalt of the bis(thio-hydrazide amide).In some embodiments, a method of preparing a bis(thio-hydrazide amide) disalt includes the steps of combining a neutral bis(thio-hydrazide amide) and an organic solvent selected from methanol, ethanol, acetone, and methyl ethyl ketone to make a mixture; adding at least two equivalents of a base selected from sodium hydroxide, potassium hydroxide, sodium methoxide, potassium methoxide, sodium ethoxide and potassium ethoxide to the mixture, thereby forming a solution; and combining the solution and methyl tert-butyl ether to precipitate the disalt of the bis(thio-hydrazide amide).The disclosed methods do not require lyophilization and the solvents used in the process can be more readily removed to low levels consistent with pharmaceutically acceptable preparation.
Source: USPTO / EPO open patent data. Objective bibliographic and citation counts.